Process of making a composition for producing irritating gas



UNITED, STATES PATENT OFFICE NIcnoLAs E. OGLESBY ND DAY'EHRENFELD, or Eneiiwoon, MARYLAND, ASSIGNOBS,

BY NES E ASSIGNMENTS, r0 FEDERAL LABORATORIES, INC, on rrrrsnoasn, PE N- SYLV NIA, A coRronA'rIoNpr DELAWARE PROCESS or MAKING A COMPOSITION FOR rnonocme mm'rAriNe GAS No Drawing. Application filed April 30, 1924, Serial No. 710,171; Renewed December 26, 1980.

(GRANTED UNDER THE Ac'r or nAacn' s, 1883, As ay Aran. a0, 1928; 870 0. 6.757

This invention described herein may be manufactured and used by or for the Government for governmental purposes without the payment to us of any royalty thereon in accordance with the act of March 3, 1883, as amended by the act of April 30, 1928.

This invention relates to a process of making a composition for producing an irritating gas used in devices such as shells, grenades,- 10 candles, etc.

Among the objects ofthis invention is the production of-a composition which may be employed in devices such as as shells, gre

nades, candles, etc. for producing an irritat- 16 inggas, which composition will remain stable and undergo practically no decomposition and generate the irritating-gas a highly eflicient method whereby substantially no decomposition of the gas will'occu'r upon its 80 neration. i

I A still further'object of this invention con sists in a method of loading devices such as shells, grenades and candles, with a coinposition which will produce an irritating gas 3 when the device functions, and which device will not explode when fired. A I

In carryln out our invention, we employ an irritant, or example capsaicin or diphenylchlorarsine, or more preferably an irao ritant which is also lac'hrymating, for example chloracetophenone, bromacetophenone or iodoacetophenone and add to this irritant an explosive fuel, for example a mixture of nitroglycerine). There is usually added to this mixture for the purpose of stabilization an anti-acid, such as MgO and ZnO, which tends to overcome or counteract the tendency be satisfied if an eflicient device and satisfactory operation areto be obtained:

1. Flashing or ignition at the orifice with consequent burning when the 'volatilized mixture comes in contact with the air should ammonium nitrate and charcoal, black powder, nitrocellulose (smokeless powder) or' ballistite (a solid solution of nitrocellulose indevices, the following requirements should be avoided-since this will decompose the irri tant anddestroy its effectiveness for the purpose desired. 7

2. Bursting of the container should be avoided. 5

3. There should be simple and positive ignition of the mixture.

In filling the grenade, candle, or shell,

loose mixtures do notgive the best results.

' For example, in grenades the loose mixtures will at times cover or plug the orifices with which these grenades are rovided and thus cause the grenade to explo e upon generation of gases therein. In order to avoid these explosions, the mixtures shouldbe rwell caked.

In loading'ia grenade or similar device with mixture of capsaicin or chloracetophenone with fuels, such as ammonium nitrate and charcoal, pressure alone may be used for the cakin operation and the exposed end of the c with some good binding material, such as a solution of shellac, in orderto revent break ing up of the cake under con ftionsbf handling and use.

e is preferably painted osition of the irritant whenemploying a,

uel such as black powder, orammonium nitrate and charcoal, we prefer to use the irri ballistite. When. 4 employing, mixtures of chloracetophenone and "smokelesspower, if

sired, and likewisethere is present thedanger of the partsiof the mixture breaking loose and covering the" holes provided for the escape of gases from these devices, thus causing the grenade or similar device to explode when fired. Some of the methods of over coming these difliculties under various conditions are as'follows: H I 'A. The. chloracetophenone, small calibre smokeless powder (.30 cal. rifle powder is quite satisfactory) and MgO are intimately mixed and the required amount of the mixture is'tamped into the container, and a solvent for .the'smokeless powder, such as acetone, is poured uniformly over the top of I tant with a fuel such as nitrocellulose or- I J 75 Owing to the greater tendency for decomv the mixture in suflicient amount to thoroughly moisten the mixture for a depth of to 1 inch and the mixture is again 'tamped. When dry, the top of the mixture is hard, compact and'firm.

B. A mixture of choracetophenone, smokeless powder and MgO is intimately mixed as under (A), and the required amount placed in the container. The container is then heated and the mixture ressed or tamped until compact. The heating should be suflicient to melt'the chloracetophenone in order that the mixturewill tamp or press compactly, but

-overheating should be avoided as this will result in a solution of smokeless powder in chloracetophenone, which will not remain.-

, fluid at orbelow 100 C. andthe mixture will not press or pack well. This method of loading is preferable to that described under (A), since the cake produced under (A) has a tendency to break up on set back when fired from a rifle because only the top surface of the cake is firmly bound. Likewise evolution of gas from grenades loaded by method (hA) is not uniform which is probably due to t e difliculty of uniformly evaporating the acetone that is added during the process.

The method of loading under (B) is rapid and ery satisfactory and particularly adapted for devices of small cross-section, but since the mixture is a poor heat conductor, this method of loading will not operate where containers of large sectional area are empended MgO. While the mixture is hot andployed, forexample certain smoke candles and large shells. w t v a v C. In this method of loading, the MgO is stirred into molten chloracetophenone and the small calibre smokeless powder, preferably heated, is added and thoroughly mixed with the molten chloracetophenone and susplastic it is pressed into the container. This method has been found very satisfactory for chloracetophenone smoke candles having a diameter of about 4 inches. -When this mixture is pressed into the candle, on cooling substantial contraction takes place and the cooled mass will not fill the container, thus result-' ing in a substantial increase of surface exposed to burning. This space should be filled either with molten chloracetophenone, paraffin; .or other material which is either inert powder of large calibre (12-inch rifle powder is satisfactory) is stacked in layers in the shell, warmed and then molten chloracetodesired to increase the ratio of smokeless powder to chloracetophenone in the mixture and thereby increasethe speed of burning or evolution of the chloracetophenone, small calibre powder may be introduced between the large blocks or cakes before adding the molten chloracetophenone.

E. In some devices, due to the irregular shape of the container,-regular stacking of the blocks of smokeless powder cannot readily be done. 'A satisfactory method for loading such containers consists in stirring MgO into molten chloracetophenone and then adding warm smokeless powder thereto, the mixture being kept stirred until cold. By this procedure a granular form of material is obtained, wherein each grain of powder is coated with chloracetophenone. The granular material is thentampedor pressed into the container and the top of the mixture covered with a layer'of a hot, plastic mixture of chloracetophenone, smokeless powder and MgO. When cold, this layer holds the filling in place.

F, Another very satisfactory method of loading consists in mixing thoroughly warm smokeless powder, MgO and molten chloracetophenone and then pressing the mass into cakes or blocks by means of dies of suitable size and shape. These cakes or blocks are then dipped in a bath of molten chloracetophenone and thenslipped into the container which is made to closely lit the cake or block. The purpose of dipping the block in the molten chloracetophenone is to provide an outer'surface of chloracetophenone on'the block which serves to prevent burning down thesides of the block. A device loaded in this manner will give, a uniformevolution of irritating or lachrymating gas without explosion of the device.

- For positive ignitionof the mixture of irritant, fuel and stabilizer, considerable heat is necessary and a composition known as a starter is employed therefor. This starter may be held in a separate tube or container and allowed to melt through and ignite the mixture. However, if the starter is carried in a tube which melts and'produces a. slag, this slag will tend to ignite the chloracetophenone vapors, causing what is known as flashing. Also, if-the starter is held in a weak container, such as paper, it has a tendency to blow through thecontainer and the ignition isnot satisfactory.

We have overcome the disadvantages incident to the use of a starter in a separate tube by binding the starter directly to the mixture.-

A suitable startercomposition for this purpose consists of meal powder (fuse powder or very finely-divided black powder) which is bound with celluloid dissolved in acetone. This starter operates very satisfactorily with mixtures having a high ratio of powder to chloracetophenone (as is the case with grenades), but when operating. with mixtures of lower ratios of powder to chloracetophenone, as'for instance the candles, iron oxide and F eS are added to the meal powder and the-mixed starter is bound to the chloracetophenone-smokeless powder-MgO mixture with celluloid dissolved in acetone. The use of a solvent for nitrocellulose or, smokeless powder binds the starter to the powder in the v chloracetophenone-smokeless powder-MgO mixture.

To ignite the starter used in our devices, the spit from ordinary safety fuses, the flash from a match head or any similar spit or flash may beemployed in connection with an suitable firing mechanism. A suitable starter composition for use with mixtures having a high ratio of powder to chloracetophenone, especially where small calibre powder is used, may be'made from substantially equal parts of mealpowder and a 3 /27 Solution of celluloid dissolved in acetone. For mixtures of low ratioof powder to chloracetophenone a suitable starter paste may be made by thoroughly mixing 2 parts .of a. dry starter to 1 part of a binding solution, the dry starter consisting of;

Fe 100 mesh) 1 part Hammer scale or iron om'de (80 mesh) 3 1 part Meal powder 2 parts The binding solution may consist of a solution of celluloid in acetone of about 4%.

In using mixtures of nitrocellulose and chloracetophenone, the proportions may vary from 1 t0 5. parts of nitrocellulose for 1 part of chloracetophenone. If MgO is employed as a stabilizer it should preferably vary from about 8 to 12% of the weight of chloracetophenone used in the mixture. i

In addition to the methods heretofore described, the'cake of fuel may be prepared In the following claims, the term gas is used to include substances which are in the gaseous phase as well as substances which are commonly termed smokes, clouds, vapors, mists, etc. and combinations of these.

The present invention is not limited to the specific details set forth in the foregoing examples which should be construed as illustrative and not by way of limitation, and in view of the numerous modifications which may be efi'ected therein without departing from the spirit and scope of this invention it is desired that only such limitations be imposed as are indicated in the appended claims. 'We claim as our invention:

1. In a process of making a composition for producing an irritating gas, molding ahej'ated mass of-a liquefied irritant which is solid at ordinary temperatures, an intimately distributed fuel which burns at a temperature suflicient t-o volatilize the irritant but below that at which the irritant will decompose within the time required for said volatilizaproducing an irritating gas comprlsingintimately mixing a fuel, an irritant, solid at ordinary temperatures, a composition to retard the combustion of the irritant and fuel mixture, coating the mixture with a volatile solvent, and evaporating the solvent.

4. In a process of, making a composition for producing an irritating gas, thoroughly mixing warm smokeless powder and magnesium oxide with molten chloracetophenone, molding the heated mixture intocakes, and dipping said molded cakes i'nto liquefied chloracetophenone.

' NICHOLAS E. OGLESBY.

7 DAY EHRENFELD.

without the aid of heat, and if it is desired to mix, the materials in the cold and without previously melting or liquefying one or more of the components, the irritant and the fuel in (1 form, with or without a stabilizer, may be treated with a solution of an adhesive or binder, for example glue, or preferably a binder of low melting point for example paraffin, pitches or bituminous materials, and the mass placed in the container, tamped and allowed to dry. The methods heretofore described which employ heat or molten materi- A .als are, however, preferable in most instances to this cold proces.

CQERTIFICATE, or comc'rioN.

Patent No. 1,864,754. v June 28, 1932.

NICHOLAS E. OGLESBY ET AL.

lit is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as follows: Page 3, line 99, claim 2, for "an read said; same page, strike out lines 101 to 107, comprising claim 3, and tor claim number "4" in line 108, read 3; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record of the case in the Patent Office.

Signed and sealed this 6th day of September, A. D. 1932.

I M. .i.'Moore, (Seal) u Acting Connniss'ioner of Patents. 

